CN106483227B - The method of quality control of Taohe Chengqi decoction composition - Google Patents
The method of quality control of Taohe Chengqi decoction composition Download PDFInfo
- Publication number
- CN106483227B CN106483227B CN201610855317.2A CN201610855317A CN106483227B CN 106483227 B CN106483227 B CN 106483227B CN 201610855317 A CN201610855317 A CN 201610855317A CN 106483227 B CN106483227 B CN 106483227B
- Authority
- CN
- China
- Prior art keywords
- solution
- taohe chengqi
- chengqi decoction
- retention time
- peak
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/60—Construction of the column
- G01N30/6052—Construction of the column body
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses the method for quality control of Taohe Chengqi decoction composition, belong to Analysis of Chinese Traditional Medicine field.The method of the present invention includes establishing Taohe Chengqi decoction composition finger-print, chromatographic condition using high performance liquid chromatography are as follows: chromatographic column is used using octadecylsilane chemically bonded silica as filler；Detecting instrument uses UV detector, Detection wavelength 210nm~250nm of finger-print；Flow velocity 0.9ml/ml~1.1ml/ml, column temperature: 25 DEG C~35 DEG C, Detection wavelength 210nm~250nm, number of theoretical plate is calculated by catechin peak should be not less than 3000, using methanol as mobile phase A, using 0.1% phosphoric acid solution as Mobile phase B, gradient elution: the gradient condition of finger-print detection elution is carried out in the following order
Description
Technical field
The invention belongs to Analysis of Chinese Traditional Medicine fields, and in particular to the method for quality control of Taohe Chengqi decoction composition.
Background technique
Traditional Chinese herbal decoction is the mainstream of clinical application, but because rise decoct, it is inconvenient to carry, decoct the decoction quality of preparation often
Because of people, there are larger differences due to decocting utensil, and classics recipe clinical efficacy is definite, Yin Jian, just, test, Lian Ershen is by vast
Consumer likes, Chinese materia medica preparation easy to carry, convenient for taking is held in classics recipe exploitation with modern science and technology, is not only
Succession to traditional Chinese medicine, and preferably promote the clinical application of classics recipe.Preparation Technology of Granules is relatively easy, is easy to assign
Shape is taken, is easy to carry, the most consistent with traditional decoction in form taking, can be compared with the spy of the holding traditional decoction of limits
Point, therefore the classics recipe selection granule taken in the form of decoction is most appropriate.The exploitation of granule should follow " Normal juice original
The principle of taste " clearly decocts standard (benchmark) decoction of parameter, to base under prior art conditions by research preparation first
The Key Quality attribute of quasi- decoction is studied, mainly with the solid content of single-prescription standard decoction (dry cream rate), finger-print, more
Index components instruct the development of particle as quality reference.Quality difference existing for medicine materical crude slice in research for reduction separate sources
Agreement is affected, the mode of selection retinue control decocts at least 10 portions of standard soup using with a batch of medicine materical crude slice
Agent, using the mean value of its Key Quality as " benchmark " of Preparation Technology of Granules parameter development.The present invention uses finger-print skill
Art measures the mode of multi-target ingredient to Taohe Chengqi decoction standard decoction (hereinafter referred to as the first peach in conjunction with multi-wavelength handoff technique
Core CHENGQI TANG composition), the quality of Taohe Chengqi decoction standard particle (hereinafter referred to as the second Taohe Chengqi decoction composition) carry out it is complete
Face evaluation.
Taohe Chengqi decoction comes from Han dynasty treatise on Febrile Diseases, by the party by peach kernel, rheum officinale, Radix Glycyrrhizae, ramulus cinnamomi, saltcake traditional Chinese medicine of the five flavours group
At curing mainly and become silted up under blood-breaking, purge heat by silt, modern clinic Chang Fangchang adds and subtracts treatment acute pelvitis of pelvic cavity with disease, adnexitis, acute brain go out
The symptoms such as blood, ovarian cyst, intrauterine Endometriosis；The upper, middle and lower coke of clinically often plus-minus treatment " stagnation of blood stasis and heat " at present
Illness；In Japan, Taohe Chengqi decoction sells ranking the 6th in pharmacy as Chinese prescription medicine, and therefore, the party has stronger exploitation
Value.
Taohe Chengqi decoction composition is made of peach kernel, rheum officinale, Radix Glycyrrhizae, ramulus cinnamomi, saltcake traditional Chinese medicine of the five flavours, is cured mainly and is become silted up under blood-breaking,
It purges heat by silt, modern clinic Chang Fangchang adds and subtracts treatment acute pelvitis of pelvic cavity, adnexitis, acute cerebral hemorrhage, ovarian cyst, uterus with disease
The symptoms such as interior Endometriosis；The illness of the upper, middle and lower coke for the treatment of " stagnation of blood stasis and heat " is clinically often added and subtracted at present；In Japan, the party
Ranking the 6th is sold in pharmacy as Chinese prescription medicine, therefore, the party has stronger Development volue.In order to more comprehensively, effectively
The quality control level and international joint for controlling Chinese medicine composition, allow clinical application safety and curative effect to be guaranteed, need
More advanced quality control method is used to Chinese medicine composition.
" Taohe Chengqi decoction " tradition drug formulation is water decoction, in order to preferably play the clinical efficacy of Taohe Chengqi decoction,
Medical personal has carried out a large amount of research to the classics side, has mainly made extensive work to its Clinical pharmacological efficiency, to it
Quality research report is less；As the compound preparation containing traditional Chinese medicine of the five flavours, contained flavour of a drug are more, have the characteristics that multicomponent, more targets,
For major part compound Chinese medicinal preparation in content control upper basic only one or two indices ingredient, quality control is single at present,
Index is few, it is difficult to the quality condition of reflection product comprehensively.It is deposited in control product quality comprehensively in view of current method of quality control
In deficiency, while due to containing the larger ingredients of physicochemical property differences such as phenolic acid class, flavonoids in Taohe Chengqi decoction, if for each
The independent method for building up measurement of index, it is cumbersome.It is had not been reported in the research of Taohe Chengqi decoction overall quality control method at present,
It is had not been reported in the research that the quality of Taohe Chengqi decoction composition controls, therefore this field needs a kind of Taohe Chengqi decoction at present
The method or equipment of the quality control of composition.
Summary of the invention
The technical problem to be solved in the present invention is that compound Chinese medicinal preparation in the prior art is overcome to control upper base in content
This only one or two indices ingredient, quality control is single, and index is few, it is difficult to which reflection flavour of a drug are more comprehensively, and component is more, target
The defect of the quality condition of more Taohe Chengqi decoction compositions, to provide the method for quality control of Taohe Chengqi decoction composition.
For this purpose, the invention provides the following technical scheme:
The method of quality control of Taohe Chengqi decoction composition, including Taohe Chengqi decoction group is established using high performance liquid chromatography
Close object finger-print, chromatographic condition are as follows:
Chromatographic column uses octadecylsilane chemically bonded silica chromatographic column；
Flow velocity 0.9ml/ml~1.1ml/ml, column temperature: 25 DEG C~35 DEG C,
Detecting instrument uses UV detector, Detection wavelength 210nm~250nm of finger-print；
Number of theoretical plate is calculated by catechin peak should be not less than 3000；
Reference solution is 50% methanol solution of catechin；
Mobile phase is that -0.1% phosphoric acid solution of methanol is system according to following eluting order progress gradient elution:
The finger-print includes 15 shared peaks: the relative retention time at each peak is respectively as follows: No. 1 peak relative retention time
It is 17.973, No. 3 peak (S) relative retention time RRT is 22.210, No. 4 peaks that RRT, which is 9.839, No. 2 peak relative retention time RRT,
Relative retention time RRT is that 24.563, No. 5 peak relative retention time RRT are that 31.572, No. 6 peak relative retention time RRT are
39.139, No. 7 peak relative retention time RRT are that 43.253, No. 8 peak relative retention time RRT are the opposite guarantor in 48.801, No. 9 peaks
It is that 60.140, No. 11 peak relative retention time RRT are that stay time RRT, which be 55.976, No. 10 peak relative retention time RRT,
61.066, S peak relative retention time RRT are that 64.647, No. 13 peak relative retention time RRT are the opposite guarantor in 67.075, No. 14 peaks
It is 71.504 that stay time RRT, which be 70.368, No. 15 peak relative retention time RRT, wherein No. 3 peaks S are the chromatographic peaks of object of reference.
Taohe Chengqi decoction composition is prepared by the following two kinds method:
(1) following medicine materical crude slice: Dan peach kernel 12g, rheum officinale 12g, radix glycyrrhizae preparata 6g, ramulus cinnamomi 6g, saltcake 6g is weighed by weight；It will
The four taste medicine materical crude slice in addition to saltcake are placed in 4L casserole, add 1400ml water, are impregnated 30 minutes, are covered, are added and boil, and are kept slightly boiled to pan-fried
Liquid 490-510ml filters out the dregs of a decoction, and saltcake is added, boils to get the first Taohe Chengqi decoction composition；Or
(2) following medicine materical crude slice: Dan peach kernel 1000g, rheum officinale 1000g, ramulus cinnamomi 500g, saltcake 500g is weighed by weight, is processed
Radix Glycyrrhizae 500g；The four taste medicine materical crude slice in addition to saltcake are added to the water of 8 times of amounts, 1.5h is decocted, obtains filtrate；Saltcake is added in filtrate, decompression
It is concentrated into the clear cream of relative density 1.05-1.15, maltodextrin is added, it is dry, it mixes, stiffened fatty acid magnesium, dry-pressing granulation is made
1000g is to get the second Taohe Chengqi decoction composition.
The Taohe Chengqi decoction composition reference solution and test solution are prepared as follows:
(1) preparation of test solution: taking the first Taohe Chengqi decoction composition 5ml, take solution, and centrifugation takes supernatant, i.e.,
?；Or the second Taohe Chengqi decoction composition 1.3g is taken, it sets in 50ml volumetric flask, is diluted with water, ultrasonic dissolution is let cool, and is added water
Constant volume shakes up, and takes solution, centrifugation, take supernatant to get；
(2) preparation of reference solution: taking catechin reference substance, and the object of reference for adding 50% methanol to be configured to 100 μ g/ml is molten
Liquid；
Sample volume is 10 μ l.
It further include using high performance liquid chromatography
Measure the anthraquinone content that dissociates in Taohe Chengqi decoction composition, chromatographic condition are as follows:
Chromatographic column uses octadecylsilane chemically bonded silica chromatographic column；
Flow velocity 0.9ml/ml~1.1ml/ml；Column temperature: 25 DEG C~35 DEG C；
Detecting instrument uses UV detector, and the Detection wavelength of finger-print is 254nm；
Number of theoretical plate is calculated by rheum emodin peak, should be not less than 3000；
Reference substance solution is the methanol solution of aloe-emodin, Rhein, rheum emodin, Chrysophanol, Physcion；
Mobile phase is that -0.1% phosphoric acid solution of methanol is mobile phase by following eluting order progress gradient elution:
Gradient elution program
When measuring dissociated anthraquinone content, test solution is made as follows: precision measures the first Taohe Chengqi decoction group
Close object 5ml be placed in 10ml volumetric flask, add methanol to dissolve and be settled to scale, shake up, take appropriate centrifugation, take supernatant to get；
Or the second Taohe Chengqi decoction composition 1.0g is taken, and it is accurately weighed, it is placed in 100ml measuring bottle, adds 50% methanol ultrasonic
Scale is dissolved and be settled to, appropriate centrifugation is taken, takes supernatant to get test solution；
Sample volume is 10 μ of μ l~20 l.
It further include using Syrups by HPLC
The content of general anthraquinone, chromatographic condition are as follows:
Chromatographic column uses octadecylsilane chemically bonded silica chromatographic column；
Flow velocity 0.9ml/ml~1.1ml/ml；Column temperature: 25 DEG C~35 DEG C；
Detecting instrument uses UV detector, and the Detection wavelength of finger-print is 254nm；
Number of theoretical plate is calculated by rheum emodin peak should be not less than 3000；
Reference substance solution is the methanol solution of aloe-emodin, Rhein, rheum emodin, Chrysophanol, Physcion；
Mobile phase is that -0.1% phosphoric acid solution of methanol is mobile phase according to following eluting order progress gradient elution:
When measuring total anthraquinones content, test solution is made as follows: taking the first Taohe Chengqi decoction composition 30ml
Or fixed second Taohe Chengqi decoction composition 1.0g, the hydrochloric acid or 8% hydrochloric acid solution 30ml of 9ml is added, dissolves, shakes up；It is added
Chloroform 40ml flows back, and takes out, cooling, extracts, and removes water, dry, and methanol dissolution is added, filters to get general anthraquinone test sample
Solution；
Measurement general anthraquinone sample volume is 10 μ l.
It further include with the content of Syrups by HPLC amarogentin, cinnamic acid, glycyrrhizic acid, chromatographic condition are as follows:
Chromatographic column uses octadecylsilane chemically bonded silica chromatographic column；
Flow velocity 0.9ml/ml~1.1ml/ml；Column temperature: 25 DEG C~35 DEG C；
Detecting instrument uses UV detector, and the Detection wavelength of finger-print is 210nm~278nm；
Number of theoretical plate is calculated by amarogentin peak should be not less than 3000；
Reference substance solution is the methanol solution of amarogentin, cinnamic acid, glycyrrhizic acid；
Mobile phase is that -0.1% phosphoric acid solution of methanol-acetonitrile is mobile phase according to following eluting order progress gradient elution:
Test solution is made as follows: precision measures the first Taohe Chengqi decoction composition 5ml and is placed in 10ml capacity
Bottle in, add methanol to dissolve and be settled to scale, shake up, take appropriate centrifugation, take supernatant to get；Or take the second Taohe Chengqi decoction
Composition 1.0g, it is accurately weighed, be placed in 100ml measuring bottle, add 50% methanol ultrasonic dissolution and be settled to scale, take in right amount from
The heart takes supernatant to get test solution；
Sample volume when measuring the content of amarogentin is 10 μ l.
Technical solution of the present invention has the advantages that
1, the finger-print in the method for quality control of Taohe Chengqi decoction composition provided by the invention can reflect comprehensively
Taohe Chengqi decoction quality information more fully and effectively controls Taohe Chengqi decoction composite preparation product matter so as to reach
The purpose of amount.
2, the method for quality control of Taohe Chengqi decoction composition provided by the invention is provided using Chinese Pharmacopoeia Commission
Similarity evaluation recognizes surveyed finger-print, easy to operate, quick；Moreover, with this
The Xiang Yidu result obtained evaluates preparation finger, and conclusion is more objective, accurate.
3, the method for quality control of Taohe Chengqi decoction composition provided by the invention is by examining preparation method of test article
The instrument of finger-print is examined and measures, the conditions such as chromatographic column, mobile phase, Detection wavelength carry out the preferred of system, establish fingerprint
Map determination condition has simultaneously carried out methodological study, on the basis of to more batches of this composition finger-print testing results, gradually
Data are accumulated, reference fingerprint are proposed, as this product finger-print standard, so that reaching more comprehensively, effectively to control
The purpose of the quality of the pharmaceutical preparations processed.
4, the method for quality control of Taohe Chengqi decoction composition provided by the invention is using in Chinese Pharmacopoeia Commission's offer
Medicine chromatographic fingerprinting similarity evaluation system-computed this composition similarity, is studied through test of many times, by opposite with calculating
The method of retention time and relative peak area compares, and the evaluation conclusion obtained is almost the same, uses Chinese medicine chromatographic fingerprint figure
Compose the similarity of similarity evaluation system evaluation finger-print, easy to operate, quick, the similarity result obtained with it, to system
Agent finger-print is evaluated, and conclusion is more objective, accurate.
5, the method for quality control of Taohe Chengqi decoction composition provided by the invention is more comprehensively characterized using finger-print
The quality information of composition reflects product quality on the whole, while being directed to prescription gomi herbs, using multi-wavelength handoff technique
Establish wherein four tastes (except mineral drug saltcake can not using high performance liquid chromatograph measurement in addition to, account for content Con trolling index 100%),
Establish the content control method of effect different dissociated anthraquinones and general anthraquinone respectively for monarch drug in a prescription rheum officinale, wherein dissociated anthraquinone is for examination
Product preparation method is simple, convenient, and measurement result is accurate, reliable；The present invention consider currently available technology control compound at
Often only one or two indices ingredient on medicine, and lack finger-print general token product quality information, therefore propose
Taohe Chengqi decoction composition quality is comprehensively controlled in a manner of the control of finger-print combination multi-target ingredient content.
6, the method for quality control of Taohe Chengqi decoction composition provided by the invention proposes to use finger-print, in conjunction with more waves
Long handoff technique measurement Taohe Chengqi decoction combines the multiple index components of species.
7, the method for quality control of Taohe Chengqi decoction composition provided by the invention can mention for Taohe Chengqi decoction composition
For a kind of more comprehensive method of quality control.
Detailed description of the invention
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art
Embodiment or attached drawing needed to be used in the description of the prior art be briefly described, it should be apparent that, it is described below
Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor
It puts, is also possible to obtain other drawings based on these drawings.
Fig. 1 is rheum emodin reference substance DAD figure；
Fig. 2 is Chrysophanol reference substance DAD figure；
Fig. 3 is Rhein reference substance DAD figure；
Fig. 4 is aloe-emodin reference substance DAD figure；
Fig. 5 is Physcion reference substance DAD figure；
Fig. 6 aloe-emodin, Rhein, rheum emodin, Chrysophanol, Physcion mixing reference substance chromatogram；
Fig. 7 dissociated anthraquinone test solution chromatogram
Fig. 8 general anthraquinone test solution chromatogram
Fig. 9 amarogentin, cinnamic acid, glycyrrhizic acid mixed reference substance solution chromatogram
Figure 10 amarogentin, cinnamic acid, glycyrrhizic acid test solution chromatogram
Catechin reference solution chromatogram in Figure 11 determining fingerprint pattern
Reference fingerprint in Figure 12 determining fingerprint pattern
The continuous four batches of sample finger-prints of Figure 13 compare chromatogram
Specific embodiment
There is provided following embodiments is to preferably further understand the present invention, it is not limited to the best embodiment party
Formula is not construed as limiting the contents of the present invention and protection scope, anyone under the inspiration of the present invention or by the present invention and its
The feature of his prior art is combined and any and identical or similar product of the present invention for obtaining, all falls within of the invention
Within protection scope.
Specific experiment step or condition person are not specified in embodiment, according to the literature in the art described routine experiment
The operation of step or condition can carry out.Reagents or instruments used without specified manufacturer, being can be by commercially available acquisition
Conventional reagent product.
Reagent of the present invention and instrument:
Reagent:
Aloe-emodin reference substance (lot number: 110795-201007, Chinese pharmaceutical biological product examine and determine research institute), rheum officinale
Sour reference substance (lot number: 110757-200206, Chinese pharmaceutical biological product examine and determine research institute), rheum emodin reference substance (lot number:
110756-200110, Chinese pharmaceutical biological product examine and determine research institute), Chrysophanol reference substance (lot number: 201118, Chinese drug is raw
Tetramune examines and determine research institute), Physcion reference substance (lot number: grind by 110758-201013, the calibrating of Chinese pharmaceutical biological product
Study carefully institute)；Amarogentin reference substance (lot number: 110820-201004, Chinese pharmaceutical biological product examine and determine research institute), cinnamic acid pair
According to product (lot number: 200503, Chinese pharmaceutical biological product examines and determine research institute), glycyrrhizic acid reference substance (lot number: 110731-201116,
Chinese pharmaceutical biological product examines and determine research institute)；Methanol (Fisher Scientific, chromatographically pure), second eyeball (Fisher
Scientific, chromatographically pure), quartz sand (analyze pure, 10~40 mesh of particle size range), Taohe Chengqi decoction composition (laboratory from
System).Reagent is that analysis is pure, and water is ultrapure water.
Instrument:
Waters e2695 high performance liquid chromatograph (2998DAD detector)；1260 high performance liquid chromatograph of Agilent
(1290DAD detector)；3000 high performance liquid chromatograph of DIONEX Ultimate；Shaking table innova 4000.
Embodiment 1: the preparation of Taohe Chengqi decoction composition
First Taohe Chengqi decoction composition: following medicine materical crude slice Dan peach kernel 12g, rheum officinale 12g, radix glycyrrhizae preparata are weighed by weight
6g, ramulus cinnamomi 6g, saltcake 6g；Four taste medicine materical crude slice (in addition to saltcake) are placed in 4L casserole, add 1400ml water, are impregnated 30 minutes, are covered, with
Sogo heating plate be heating device, boil (about 25min), keep slightly boiled (about 85 minutes, evaporation capacity about 10g/min) to decocting liquid about
500ml filters out the dregs of a decoction using two layers of hospital gauze, saltcake is added, boil to get.
Second Taohe Chengqi decoction composition: following medicine materical crude slice Dan peach kernel 1000g, rheum officinale 1000g, ramulus cinnamomi are weighed by weight
500g, saltcake 500g, radix glycyrrhizae preparata 500g；Four taste medicine materical crude slice (in addition to saltcake) add the water of 8 times of amounts, decoct 1.5h, obtain filtrate；Saltcake
It is added in filtrate, being concentrated under reduced pressure into relative density is 1.05-1.15 (preferably 1.10) clear cream (60 DEG C~70 DEG C), is added appropriate
Maltodextrin, it is dry, mix, add appropriate magnesium stearate, dry-pressing granulation, be made 1000g to get.The combination of second Taohe Chengqi decoction
Object the second Taohe Chengqi decoction composition is aluminized/polyethylene composite film using polyester, and packing specification is 4.0g/ bags.
Embodiment 2.HPLC method measures the anthraquinone content that dissociates in Taohe Chengqi decoction composition
(1) chromatographic condition and system suitability
Using octadecylsilane chemically bonded silica as filler；Using acetonitrile as mobile phase A, 0.1% phosphoric acid is Mobile phase B, ladder
Degree elution；Detection wavelength is 254nm.Number of theoretical plate is calculated by rheum emodin peak should be not less than 3000, flow velocity: 1.0ml/min, column
Temperature: 30 DEG C.
Gradient elution program
(2) preparation of reference substance solution
Precision weighs aloe-emodin reference substance, Rhein reference substance, rheum emodin reference substance, Chrysophanol reference substance, rheum officinale
Plain methyl ether reference substance is appropriate, adds methanol that every 1ml is respectively prepared and contains aloe-emodin, Rhein, rheum emodin, each 80 μ g of Chrysophanol,
The solution of 40 μ g of Physcion；It is accurate respectively to measure above-mentioned each 2ml of reference substance solution, it mixes to get (aloe is contained in every 1ml
Rheum emodin, Rhein, rheum emodin, Chrysophanol each 16 μ g, 8 μ g containing Physcion).
(3) preparation of test solution
The preparation of first Taohe Chengqi decoction composition test solution: precision measures the first Taohe Chengqi decoction composition 5ml and sets
In 10ml volumetric flask, add methanol to dissolve and be settled to scale, shake up, take appropriate centrifugation, take supernatant to get；
The preparation of second Taohe Chengqi decoction composition test solution: taking the second Taohe Chengqi decoction composition 1.0g, and precision claims
It is fixed, it is placed in 100ml measuring bottle, adds 50% methanol ultrasonic dissolution and be settled to scale, take appropriate centrifugation, take supernatant to get confession
Test sample solution.
(4) selection of Detection wavelength
Take the online DAD map observation (See Figure of rheum emodin, Chrysophanol, Rhein, aloe-emodin, Physcion
1-5), five absorption curve is more consistent, referring to the assay institute of first rheum officinale recorded of " Chinese Pharmacopoeia " version in 2010
The Detection wavelength of rheum emodin, Chrysophanol, Rhein, aloe-emodin, Physcion is set to by the Detection wavelength used
254nm。
(5) measuring method precision draws reference substance solution and 20 μ l of test solution, injects liquid chromatograph, measurement to get.
(see Fig. 6-7)
(6) preparation of standard curve
Precision weighs five reference substances, be configured to respectively aloe-emodin be configured to concentration be 64.719,32.360,
16.180, the reference substance solution of 8.090,0.809,0.404 and 0.202 μ g/ml；Rhein be configured to concentration be 188.559,
94.280, the reference substance solution of 47.14,23.570,2.357,1.178 and 0.589 μ g/ml；Rheum emodin is configured to concentration
66.340, the reference substance solution of 33.170,16.585,8.293,0.829,0.415 and 0.207 μ g/ml；Chrysophanol is configured to dense
Degree is the reference substance solution of 104.435,52.218,26.109,13.054,1.305,0.653 and 0.326 μ g/ml；Rheum emodin first
Ether is configured to the reference substance solution that concentration is 39.042,19.521,9.760,4.880,0.488,0.244 and 0.122 μ g/ml；
10 μ l of sample introduction respectively, measurement record chromatogram.With concentration (C) for abscissa, peak area (A) is ordinate, with concentration to average
Peak area carries out regression analysis, draws standard curve.10 μ l of sample introduction respectively, measurement record chromatogram.With concentration (C) for horizontal seat
Mark, peak area (A) are ordinate, carry out regression analysis to average peak area with concentration, draw standard curve.Aloe-emodin
Equation of linear regression are as follows: A=1.1833C+0.0954, r=1.0000 are 0.202~64.719 μ gml in concentration-1Range
Interior, linear relationship is good, the equation of linear regression of Rhein are as follows: A=1.0031C+0.2059, r=1.0000 are in concentration
0.589~188.559 μ gml-1In the range of, linear relationship is good, the equation of linear regression of rheum emodin are as follows: A=0.8559C+
0.0607, r=1.0000, it is 0.207~66.340 μ gml in concentration-1In the range of, linear relationship is good, the line of Chrysophanol
Property regression equation are as follows: A=1.2195C+0.1586, r=1.0000, concentration be 0.326~104.435 μ gml-1Range
Interior, linear relationship is good, the equation of linear regression of Physcion are as follows: A=0.8734C+0.0341, r=1.0000, in concentration
For 0.122~39.042 μ gml-1In the range of, linear relationship is good.Test solution and reference substance solution used in this product
Concentration is within this range.
(7) methodological study and sample measurement
The measuring method passes through methodology validation, and negative sample is noiseless to measurement result, and stability of the sample in 48h is good
Good, five index RSD values of dissociated anthraquinone respectively are: 0.2%, 0.4%, 0.3%, 0.7%, 0.9%；Repeatability measurement knot
Five index RSD values of fruit are respectively 0.5%, 0.7%, 0.6%, 0.8%, 1.5%；Five index mean sample recovery rate difference
Are as follows: aloe-emodin 99.1% (n=9), RSD% 1.3%；Rhein 99.3% (n=9), RSD% 1.3%；Rheum emodin
100.3% (n=9), RSD% 1.0%；Chrysophanol 99.9% (n=9), RSD% 1.3%, Physcion 100.3%
(n=9), RSD% 2.6%.Show that method accuracy is high, repeatability is good.10 the first peach-pits of batch are measured with this method to hold
The dissociated anthraquinone content of gas soup composition and continuous the second Taohe Chengqi decoction of four batches composition is as a result as follows:
1 10 batches of the first Taohe Chengqi decoction compositions of table and continuous the second Taohe Chengqi decoction of four batches composition dissociated anthraquinone
Content results
(8) first Taohe Chengqi decoction compositions require every part of decoction liquor, the second every 4g of Taohe Chengqi decoction composition requirement to contain
Amount, the two dissociated anthraquinone must not be less than 1.4mg.
Embodiment 3.HPLC method measures total anthraquinones content in Taohe Chengqi decoction composition
(1) chromatographic condition and system suitability
Using octadecylsilane chemically bonded silica as filler；Using methanol as mobile phase A, 0.1% phosphoric acid is Mobile phase B, ladder
Degree elution；Detection wavelength is 254nm.Number of theoretical plate is calculated by rheum emodin peak should be not less than 3000, flow velocity: 0.8ml/min, column
Temperature: 30 DEG C.
Gradient elution program
(2) preparation of reference substance solution
Precision weighs aloe-emodin reference substance, Rhein reference substance, rheum emodin reference substance, Chrysophanol reference substance, rheum officinale
Plain methyl ether reference substance is appropriate, adds methanol that every 1ml is respectively prepared and contains aloe-emodin, Rhein, rheum emodin, each 80 μ g of Chrysophanol,
The solution of 40 μ g of Physcion；It is accurate respectively to measure above-mentioned each 2ml of reference substance solution, it mixes to get (aloe is contained in every 1ml
Rheum emodin, Rhein, rheum emodin, Chrysophanol each 16 μ g, 8 μ g containing Physcion).
(3) preparation of test solution
The preparation of first Taohe Chengqi decoction composition test solution: the first Taohe Chengqi decoction composition 30ml is taken to be placed in
In 250ml boiling flask, the hydrochloric acid or 8% hydrochloric acid solution 30ml, ultrasonic dissolution that 9ml is added are shaken up；Chloroform is added
40ml, 95 DEG C of reflux 1h (paying attention to that a small amount of quartz sand is added when reflux), takes out, cooling, with chloroform machinery shaking out three
Secondary, each 30ml merges chloroform, anhydrous sodium sulfate water removal, and water-bath volatilizes, and 25ml methanol, dissolution is added in precision；It takes appropriate
The miillpore filter for crossing 0.45 μm takes subsequent filtrate to get general anthraquinone test solution.
The preparation of second Taohe Chengqi decoction composition test solution: taking the second Taohe Chengqi decoction composition 1.0g, and precision claims
It is fixed, 8% hydrochloric acid solution 30ml is added, ultrasonic dissolution shakes up；Chloroform 40ml is added, 95 DEG C of reflux 1h (pay attention to adding when reflux
Enter a small amount of quartz sand), it takes out, cooling, three times with the shaking out of chloroform machinery, each 30ml merges chloroform, anhydrous
Sodium sulphate water removal, water-bath volatilize, and 25ml methanol, dissolution is added in precision；The miillpore filter for taking 0.45 μm excessively in right amount, takes subsequent filtrate,
Up to general anthraquinone test solution.
(4) measuring method precision draws reference substance solution and 10 μ l of test solution, injects liquid chromatograph, measurement to get.
(see Fig. 8)
(5) preparation of standard curve
Precision pipettes reference substance stock solution, dilution, aloe-emodin be configured to concentration be 81.438,40.719,20.360,
10.180, the reference substance solution of 1.018,0.509,0.254 and 0.127 μ g/ml；Rhein be configured to concentration be 236.176,
118.088, the reference substance solution of 59.044,29.522,2.952,1.476,0.738 and 0.369 μ g/ml；Rheum emodin is configured to
Concentration is the reference substance solution of 86.320,43.160,21.580,10.790,1.079,0.540,0.270 and 0.135 μ g/ml；
It is 133.270,66.635,33.318,16.659,1.666,0.833,0.416 and 0.208 μ g/ml that Chrysophanol, which is configured to concentration,
Reference substance solution；Physcion be configured to concentration be 51.297,25.649,12.824,6.412,0.641,0.321,
The reference substance solution of 0.160 and 0.080 μ g/ml.10 μ l of sample introduction respectively, measurement record chromatogram.With concentration (C) for abscissa,
Peak area (A) is ordinate, carries out regression analysis to average peak area with concentration, draws standard curve.The line of aloe-emodin
Property regression equation are as follows: A=1.1834C+0.0952, r=1.0000, concentration be 0.127~81.438 μ gml-1Range
Interior, linear relationship is good, the equation of linear regression of Rhein are as follows: A=1.0028C+0.1861, r=1.0000 are in concentration
0.369~236.176 μ gml-1In the range of, linear relationship is good, the equation of linear regression of rheum emodin are as follows: A=0.8558C+
0.0689, r=1.0000, it is 0.135~86.320 μ gml in concentration-1In the range of, linear relationship is good, the line of Chrysophanol
Property regression equation are as follows: A=1.2195C+0.1801, r=1.0000, concentration be 0.208~133.270 μ gml-1Range
Interior, linear relationship is good, the equation of linear regression of Physcion are as follows: A=0.8734C+0.0360, r=1.0000, in concentration
For 0.080~51.297 μ gml-1In the range of, linear relationship is good, and reference substance used in this product general anthraquinone, the sample introduction of sample are dense
Degree is within this range.
(6) methodological study and sample measurement
The measuring method passes through methodology validation, and negative sample is noiseless to measurement result, and stability of the sample in 40h is good
Good, five index RSD values of general anthraquinone respectively are: 0.4%, 0.4%, 0.3%, 0.3%, 0.6%；Repeated measurement result
Five index RSD values are respectively 1.0%, 1.3%, 1.1%, 1.8%, 1.5%；Five index mean sample recovery rate difference
Are as follows: aloe-emodin 99.4% (n=9), RSD% 2.4%；Rhein 99.5% (n=9), RSD% 2.8%；Rheum emodin
99.4% (n=9), RSD% 2.5%；Chrysophanol 98.2% (n=9), RSD% 2.4%, 98.0% (n of Physcion
=9), RSD% 3.1%.This method accuracy is high, and repeatability is good.10 the first Taohe Chengqi decoctions of batch are measured with this method
The total anthraquinones content of composition and continuous the second Taohe Chengqi decoction of four batches composition, as a result as follows:
210 batches of the first Taohe Chengqi decoction compositions of table and continuous the second Taohe Chengqi decoction of four batches composition total anthraquinones content
As a result
(7) first Taohe Chengqi decoction compositions require every part of decoction liquor, the second every 4g of Taohe Chengqi decoction composition requirement to contain
Amount, the two general anthraquinone must not be less than 6.7mg.
Embodiment 4.HPLC method measures amarogentin, cinnamic acid, glycyrrhizic acid content in Taohe Chengqi decoction composition
(1) chromatographic condition and system suitability
Using octadecylsilane chemically bonded silica as filler, using methanol as mobile phase A, acetonitrile is Mobile phase B, 0.1% phosphorus
Acid is mobile phase C, and according to the form below carries out gradient elution, flow velocity: 1.0ml/min, column temperature: 30 DEG C, number of theoretical plate presses amarogentin peak
3000 should be not less than by calculating.
Gradient elution program
Detection wavelength table
(2) preparation of reference substance solution
Cinnamic acid, amarogentin, appropriate ammonium glycyrrhetate are taken, is prepared into every ml 120 μ g containing amarogentin, meat with 50% methanol
10 μ g of cinnamic acid, the mixed reference substance solution of 80 μ g of ammonium glycyrrhetate.
(3) preparation of test solution
The preparation of first Taohe Chengqi decoction composition test solution: precision measures the first Taohe Chengqi decoction composition 5ml and sets
In 10ml volumetric flask, add methanol to dissolve and be settled to scale, take appropriate 12000r/min centrifugation 10min, take supernatant to get
Test solution.
The preparation of second Taohe Chengqi decoction composition test solution: taking the second Taohe Chengqi decoction composition 1.0g, and precision claims
It is fixed, it is placed in 100ml measuring bottle, 50% methanol ultrasonic dissolution is simultaneously settled to scale, takes appropriate 12000r/min centrifugation 10min, takes
Supernatant is to get test solution.
(4) measuring method
It is accurate respectively to draw reference substance solution and each 10 μ l of test solution, inject liquid chromatograph, measurement to get.(see
Fig. 9-10)
(5) preparation of standard curve
According to reference substance solution preparation method, take amarogentin reference substance, be configured to concentration be 6.400,12.800,
25.601, the reference substance solution of 51.202,102.404,204.808,409.615 and 819.230 μ g/ml；Cinnamic acid is configured to
Concentration is the reference substance solution of 1.156,2.311,4.623,9.245,18.490,36.980,73.960 and 147.920 μ g/ml；
It is 1.855,3.710,7.420,14.840,29.680,59.361,118.721 and 237.443 μ g/ that glycyrrhizic acid, which is configured to concentration,
The reference substance solution of ml.10 μ l of sample introduction respectively, measurement record chromatogram.With concentration (C) for abscissa, peak area (A) is vertical sits
Mark carries out regression analysis to average peak area with concentration, draws standard curve.Amarogentin equation of linear regression are as follows: A=
0.1108C+0.1385, r=1.0000, linear relationship are good；Cinnamic acid equation of linear regression are as follows: A=0.9656C+0.0812,
R=1.0000, linear relationship are good；Glycyrrhizic acid equation of linear regression are as follows: A=0.1032C+0.0224, r=1.0000, linearly
Relationship is good.According to standard curve, the range of linearity of amarogentin concentration is 6.400~819.230 μ gml-1, cinnamic acid is dense
The range of linearity of degree is 1.156~147.920 μ gml-1, the range of linearity of Radix Glycyrrhizae acid concentration is 1.855~237.443 μ g
ml-1, this product reference substance and test solution concentration are within this range.
(6) methodological study and sample measurement
The measuring method passes through methodology validation, and negative sample is noiseless to measurement result, and stability of the sample in 40h is good
Good, three index RSD values respectively are: 0.2%, 0.5%, 0.3%；Five index RSD value difference of repeated measurement result
It is 0.9%, 0.6%, 1.0%；Three index mean sample recovery rates are respectively as follows: amarogentin 96.8% (n=9), and RSD% is
1.3%；Cinnamic acid 97.7% (n=9), RSD% 1.1%；Glycyrrhizic acid 100.1% (n=9), RSD% 0.9%.This method
Accuracy is high, and repeatability is good.10 batch the first Taohe Chengqi decoction compositions and continuous the second peach of four batches are measured with this method
The content of three indexs of core CHENGQI TANG composition is as a result as follows:
3 10 batches of the first Taohe Chengqi decoction compositions of table and three indexs of continuous the second Taohe Chengqi decoction of four batches composition
Content results
(7) first Taohe Chengqi decoction compositions require every part of decoction liquor, the second every 4g of Taohe Chengqi decoction composition requirement to contain
Amount, the two amarogentin must not be less than 34.7mg, and cinnamic acid must not be less than 1.5mg, and glycyrrhizic acid must not be less than 7.7mg.
Embodiment 5.HPLC method establishes the detection method of the finger-print of Taohe Chengqi decoction composition
(1) chromatographic condition and system suitability
Using octadecylsilane chemically bonded silica as filler；It is flowing with 0.1% phosphoric acid solution using methanol as mobile phase A
Phase B, the regulation according to the form below carry out gradient elution；Flow velocity 1.0ml/ml, column temperature: 30 DEG C, Detection wavelength 230nm.Number of theoretical plate
5000 should be not less than by calculating by catechin peak.
Finger-print eluent gradient program
(2) preparation of reference solution
Take catechin reference substance appropriate, add 50% methanol be configured to the reference solution of 100 μ g/ml to get.(see Figure 11)
(3) preparation of test solution
Take the first Taohe Chengqi decoction composition 5ml, 12000r/min to be centrifuged 10min, take supernatant to get；Or take second
Taohe Chengqi decoction composition 1.3g, sets in 50ml volumetric flask, is diluted with water, and ultrasonic dissolution is let cool, and adds water constant volume, is shaken up, and takes
Solution, 12000r/min be centrifuged 10min, take supernatant to get
(4) measuring method is accurate respectively draws reference solution and each 10 μ l of test solution, injects liquid chromatograph, surveys
It is fixed to get.
(5) determination of Taohe Chengqi decoction composition reference fingerprint and similarity analysis
Using same batch medicine materical crude slice, 10 parts of the first Taohe Chengqi decoction composition is prepared, respectively the combination of the first Taohe Chengqi decoction
Object test solution is measured by determining fingerprint pattern method, records map.By analysis, determine its common characteristic peaks be 15 (see
Attached drawing 12), the relative retention time deviation RSD of 15 common characteristic peaks is respectively less than 2%, it may be assumed that
No. 1 peak relative retention time RRT is 9.839, RSD% 1.39%；
No. 2 peak relative retention time RRT are 17.973, RSD% 0.07%；
No. 3 peak (S) relative retention time RRT are 22.210, RSD% 0.04%；
No. 4 peak relative retention time RRT are 24.563, RSD% 0.05%；
No. 5 peak relative retention time RRT are 31.572, RSD% 0.04%；
No. 6 peak relative retention time RRT are 39.139, RSD% 0.03%；
No. 7 peak relative retention time RRT are 43.253, RSD% 0.02%；
No. 8 peak relative retention time RRT are 48.801, RSD% 0.02%；
No. 9 peak relative retention time RRT are 55.976, RSD% 0.02%；
No. 10 peak relative retention time RRT are 60.140, RSD% 0.01%；
No. 11 peak relative retention time RRT are 61.066, RSD% 0.01%；
12 peak (S) relative retention time RRT are 64.647, RSD% 0.01%；
No. 13 peak relative retention time RRT are 67.075, RSD% 0.01%；
No. 14 peak relative retention time RRT are 70.368, RSD% 0.01%；
No. 15 peak relative retention time RRT are 71.504.Wherein, No. 3 peaks S are the chromatographic peaks of object of reference.
Map is handled with chromatographic fingerprints of Chinese materia medica similarity evaluation software (version in 2012), using 160512-1 as ginseng
According to map, the first Taohe Chengqi decoction composition reference fingerprint is obtained.Sample similarity is calculated using Cosin method, as a result
Show 10 part of first Taohe Chengqi decoction composition similarity of decoction between 0.934~1.000, similarity is higher.
4 10 part of first Taohe Chengqi decoction composition similarity evaluation result of table
Medicine materical crude slice corresponding to the first Taohe Chengqi decoction composition is taken, continuous the second Taohe Chengqi decoction of three batches composition is prepared
Sample is measured by finger print measuring method, is recorded chromatogram (see attached drawing 13), is generated with the first Taohe Chengqi decoction composition
Reference fingerprint calculates the similarity of 4 batch the second Taohe Chengqi decoction compositions as retinue control map.As a result it sees below
Table.
Second Taohe Chengqi decoction composition similarity calculation result
(6) by similarity evaluation calculate, in terms of the peak mark, test article fingerprint with it is right
0.90 must not be lower than according to the similarity of finger-print.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (8)
1. the method for quality control of Taohe Chengqi decoction composition, which is characterized in that including establishing peach using high performance liquid chromatography
Core CHENGQI TANG composition finger-print, chromatographic condition are as follows:
Chromatographic column uses octadecylsilane chemically bonded silica chromatographic column；
Flow velocity 0.9ml/ml~1.1ml/ml, column temperature: 25 DEG C~35 DEG C,
Detecting instrument uses UV detector, Detection wavelength 210nm~250nm；
Number of theoretical plate is calculated by catechin peak should be not less than 3000；
Reference solution is 50% methanol solution of catechin；
Mobile phase is that -0.1% phosphoric acid solution of methanol is system according to following eluting order progress gradient elution:
It further include with the anthraquinone content that dissociates in high effective liquid chromatography for measuring Taohe Chengqi decoction composition, chromatographic condition are as follows:
Chromatographic column uses octadecylsilane chemically bonded silica chromatographic column；
Flow velocity 0.9ml/ml~1.1ml/ml；Column temperature: 25 DEG C~35 DEG C；
Detecting instrument uses UV detector, Detection wavelength 254nm；
Number of theoretical plate is calculated by rheum emodin peak, should be not less than 3000；
Reference substance solution is the methanol solution of aloe-emodin, Rhein, rheum emodin, Chrysophanol, Physcion；
Mobile phase is that -0.1% phosphoric acid solution of acetonitrile is mobile phase by following eluting order progress gradient elution:
It further include the content with Syrups by HPLC general anthraquinone, chromatographic condition are as follows:
Chromatographic column uses octadecylsilane chemically bonded silica chromatographic column；
Flow velocity 0.9ml/ml~1.1ml/ml；Column temperature: 25 DEG C~35 DEG C；
Detecting instrument uses UV detector, Detection wavelength 254nm；
Number of theoretical plate is calculated by rheum emodin peak should be not less than 3000；
Reference substance solution is the methanol solution of aloe-emodin, Rhein, rheum emodin, Chrysophanol, Physcion；
Mobile phase is that -0.1% phosphoric acid solution of methanol is mobile phase according to following eluting order progress gradient elution:
2. method of quality control according to claim 1, which is characterized in that the finger-print includes 15 shared peaks:
It is that No. 9.839,2 peak relative retention time RRT are that the relative retention time at each peak, which is respectively as follows: No. 1 peak relative retention time RRT,
17.973, No. 3 peak (S) relative retention time RRT are that 22.210, No. 4 peak relative retention time RRT are that 24.563, No. 5 peaks are opposite
Retention time RRT is that 31.572, No. 6 peak relative retention time RRT are that 39.139, No. 7 peak relative retention time RRT are
43.253, No. 8 peak relative retention time RRT are that 48.801, No. 9 peak relative retention time RRT are the opposite guarantor in 55.976, No. 10 peaks
It is the peak 61.066, S relative retention time RRT is 64.647,13 that stay time RRT, which be 60.140, No. 11 peak relative retention time RRT,
It is 70.368, No. 15 peak relative retention times that number peak relative retention time RRT, which is 67.075, No. 14 peak relative retention time RRT,
RRT is 71.504, wherein No. 3 peaks S are the chromatographic peaks of object of reference.
3. method of quality control according to claim 2, which is characterized in that Taohe Chengqi decoction composition presses the following two kinds side
Method preparation:
(1) following medicine materical crude slice: Dan peach kernel 12g, rheum officinale 12g, radix glycyrrhizae preparata 6g, ramulus cinnamomi 6g, saltcake 6g is weighed by weight；Awns will be removed
Four taste medicine materical crude slice outside nitre are placed in 4L casserole, add 1400ml water, are impregnated 30 minutes, are covered, are added and boil, and are kept slightly boiled to decocting liquid
490-510ml filters out the dregs of a decoction, and saltcake is added, boils to get the first Taohe Chengqi decoction composition；Or
(2) following medicine materical crude slice is weighed by weight: Dan peach kernel 1000g, rheum officinale 1000g, ramulus cinnamomi 500g, saltcake 500g, radix glycyrrhizae preparata
500g；The four taste medicine materical crude slice in addition to saltcake are added to the water of 8 times of amounts, 1.5h is decocted, obtains filtrate；Saltcake is added in filtrate, is concentrated under reduced pressure
Maltodextrin is added in the clear cream for being 1.05-1.15 to relative density, dry, mixes, stiffened fatty acid magnesium, and dry-pressing granulation is made
1000g is to get the second Taohe Chengqi decoction composition.
4. method of quality control according to claim 3, which is characterized in that the Taohe Chengqi decoction composition object of reference is molten
Liquid and test solution are prepared as follows:
(1) preparation of test solution: taking the first Taohe Chengqi decoction composition 5ml, centrifugation, take supernatant to get；Or take second
Taohe Chengqi decoction composition 1.3g, sets in 50ml volumetric flask, is diluted with water, and ultrasonic dissolution is let cool, and adds water constant volume, is shaken up, and takes
Solution, centrifugation, take supernatant to get；
(2) preparation of reference solution: taking catechin reference substance, and 50% methanol is added to be configured to the reference solution of 100 μ g/ml；
Sample volume is 10 μ l.
5. method of quality control according to claim 4, which is characterized in that when measurement dissociated anthraquinone content,
Test solution is made as follows: precision measures the first Taohe Chengqi decoction composition 5ml and is placed in 10ml volumetric flask,
Add methanol to dissolve and be settled to scale, shake up, take appropriate centrifugation, takes supernatant, i.e.,
To obtain the final product；
Or the second Taohe Chengqi decoction composition 1.0g is taken, and it is accurately weighed, it is placed in 100ml measuring bottle, adds 50% methanol ultrasonic dissolution
And it is settled to scale, appropriate centrifugation is taken, takes supernatant to get test solution；
Sample volume is 10 μ of μ l~20 l.
6. method of quality control according to claim 5, which is characterized in that when measurement total anthraquinones content,
Test solution is made as follows: taking the first Taohe Chengqi decoction composition 30ml or fixed second Taohe Chengqi decoction group
Object 1.0g is closed, the hydrochloric acid or 8% hydrochloric acid solution 30ml of 9ml is added, dissolves, shakes up；Chloroform 40ml is added, flows back, takes out,
It is cooling, it extracts, removes water, it is dry, methanol dissolution is added, filters to get general anthraquinone test solution；
Measurement general anthraquinone sample volume is 10 μ l.
7. method of quality control according to claim 6, which is characterized in that further include with Syrups by HPLC semen armeniacae amarae
The content of glycosides, cinnamic acid, glycyrrhizic acid, chromatographic condition are as follows:
Chromatographic column uses octadecylsilane chemically bonded silica chromatographic column；
Flow velocity 0.9ml/ml~1.1ml/ml；Column temperature: 25 DEG C~35 DEG C；
Detecting instrument uses UV detector, and Detection wavelength is 210nm~278nm；
Number of theoretical plate is calculated by amarogentin peak should be not less than 3000；
Reference substance solution is the methanol solution of amarogentin, cinnamic acid, glycyrrhizic acid；
Mobile phase is that -0.1% phosphoric acid solution of methanol-acetonitrile is mobile phase according to following eluting order progress gradient elution:
8. method of quality control according to claim 7, which is characterized in that test solution is made as follows: essence
The first Taohe Chengqi decoction composition 5ml of close measurement is placed in 10ml volumetric flask, is added methanol to dissolve and is settled to scale, shakes up, take
Appropriate centrifugation, take supernatant to get；Or the second Taohe Chengqi decoction composition 1.0g is taken, and it is accurately weighed, it is placed in 100ml measuring bottle,
Add 50% methanol ultrasonic dissolution and be settled to scale, takes appropriate centrifugation, take supernatant to get test solution；
Sample volume when measuring the content of amarogentin is 10 μ l.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610855317.2A CN106483227B (en) | 2016-09-27 | 2016-09-27 | The method of quality control of Taohe Chengqi decoction composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610855317.2A CN106483227B (en) | 2016-09-27 | 2016-09-27 | The method of quality control of Taohe Chengqi decoction composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106483227A CN106483227A (en) | 2017-03-08 |
| CN106483227B true CN106483227B (en) | 2019-04-12 |
Family
ID=58268049
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610855317.2A Active CN106483227B (en) | 2016-09-27 | 2016-09-27 | The method of quality control of Taohe Chengqi decoction composition |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106483227B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106483213B (en) * | 2016-09-27 | 2019-04-12 | 华润三九医药股份有限公司 | The method for building up and finger-print of Taohe Chengqi decoction composition finger-print |
| CN109223881A (en) * | 2018-09-11 | 2019-01-18 | 河北中医学院 | A method of optimization Taohe Chengqi decoction decoction preparation process |
| CN110118846B (en) * | 2019-03-26 | 2021-02-26 | 河北中医学院 | Method for establishing reference of peach pit qi-bearing soup substance |
| CN110836934A (en) * | 2019-11-22 | 2020-02-25 | 成都中医药大学 | Construction method and identification application of peach kernel and walnut kernel analytical model |
| CN113759019B (en) * | 2021-03-03 | 2023-04-28 | 北京康仁堂药业有限公司 | Evaluation method and quality control method of peach pit qi-supporting soup preparation process |
| CN113484428B (en) * | 2021-05-20 | 2023-05-05 | 广东一方制药有限公司 | Construction method of peach pit qi-bearing decoction characteristic spectrum |
| CN113484429B (en) * | 2021-05-20 | 2023-06-02 | 广东一方制药有限公司 | Method for establishing standard of peach pit qi-bearing soup material |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102114083A (en) * | 2011-01-04 | 2011-07-06 | 康美药业股份有限公司 | Fingerprint of Polygonum multiflorum and establishment method and application thereof |
| CN105044260A (en) * | 2015-06-30 | 2015-11-11 | 广州市香雪制药股份有限公司 | Yupingfeng preparation fingerprint construction method and detection method |
| CN105181867A (en) * | 2015-09-09 | 2015-12-23 | 四川绿叶宝光药业股份有限公司 | Establishment method of traditional Chinese medicine composite fingerprint |
| CN105588888A (en) * | 2016-01-13 | 2016-05-18 | 贵州百灵企业集团制药股份有限公司 | Traditional Chinese medicine fingerprint spectrum quality control and measuring method |
| CN106483213A (en) * | 2016-09-27 | 2017-03-08 | 华润三九医药股份有限公司 | The method for building up of Taohe Chengqi decoction composition finger-print and finger-print |
-
2016
- 2016-09-27 CN CN201610855317.2A patent/CN106483227B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102114083A (en) * | 2011-01-04 | 2011-07-06 | 康美药业股份有限公司 | Fingerprint of Polygonum multiflorum and establishment method and application thereof |
| CN105044260A (en) * | 2015-06-30 | 2015-11-11 | 广州市香雪制药股份有限公司 | Yupingfeng preparation fingerprint construction method and detection method |
| CN105181867A (en) * | 2015-09-09 | 2015-12-23 | 四川绿叶宝光药业股份有限公司 | Establishment method of traditional Chinese medicine composite fingerprint |
| CN105588888A (en) * | 2016-01-13 | 2016-05-18 | 贵州百灵企业集团制药股份有限公司 | Traditional Chinese medicine fingerprint spectrum quality control and measuring method |
| CN106483213A (en) * | 2016-09-27 | 2017-03-08 | 华润三九医药股份有限公司 | The method for building up of Taohe Chengqi decoction composition finger-print and finger-print |
Non-Patent Citations (4)
| Title |
|---|
| HPLC 测定桃核承气汤中蒽醌类成分;谢华等;《上海中医药杂志》;20061231;第40卷(第7期);第73-76页 |
| HPLC法测定不同产地桃仁中苦杏仁苷的含量;叶晶晶;《中华中医药学刊》;20110131;第29卷(第1期);第206-207页 |
| 桃核承气汤中桃仁不同配伍对苦杏仁苷含量的影响;黄家卫等;《浙江中医药大学学报》;20120430;第36卷(第4期);第422-424页 |
| 桃核承气汤中桃仁单煎与桃仁甘草合煎的苦杏仁苷含量变化研究;吴巧凤等;《浙江中医药大学学报》;20090930;第33卷(第5期);第738-740页 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106483227A (en) | 2017-03-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106483227B (en) | The method of quality control of Taohe Chengqi decoction composition | |
| CN106483213B (en) | The method for building up and finger-print of Taohe Chengqi decoction composition finger-print | |
| CN106226440B (en) | The method of quality control of Shengma Gegen Tang composition | |
| CN105806975A (en) | Method for establishing lonicerae and forsythiae powder UPLC fingerprint spectrum | |
| CN110118846A (en) | The method for building up of Taohe Chengqi decoction matter basis | |
| CN106053700B (en) | A kind of finger print measuring method of tuber of multiflower knotweed Cognex | |
| CN108459090B (en) | Quality control method of Jichuan decoction composition | |
| CN108459128B (en) | Quality control method of angelica sinensis Sini decoction composition | |
| CN113281439B (en) | Quality control detection method of Shenbao tablets | |
| CN104965033B (en) | Determination method for HPLC (High Performance Liquid Chromatography) fingerprint of rhizoma atractylodis and cortex phellodendri pain removing preparation | |
| CN106802327A (en) | It is a kind of to set up the method that youngster rushes down the finger-print for stopping pharmaceutical preparation | |
| CN111879884A (en) | Quality control method of Chinese medicinal preparation | |
| CN113759035A (en) | Method for constructing fingerprint of Xiaochengqi decoction | |
| CN108459129A (en) | A kind of method of quality control of Tetrandra and Poria Decoction composition | |
| CN104833751B (en) | The method for building up of XIAOER GANMAO TANGJIANG Aqueous extracts HPLC standard finger-print and application thereof | |
| CN108459091B (en) | Method for establishing fingerprint spectrum of angelica sinensis Sini decoction composition | |
| CN106526000B (en) | The method for building up and finger-print of Shengma Gegen Tang composition finger-print | |
| CN110967414A (en) | High performance liquid chromatography method for detecting fingerprint of giant knotweed medicinal material, decoction pieces, standard decoction and formula granules | |
| CN106950289B (en) | A kind of coronary disease treatment capsule one is surveyed comments detection method of content more | |
| CN109975442A (en) | A kind of fingerprint controlling wine-prepared fructus corni processing procedure parameter | |
| CN105738499A (en) | Method for constructing refined coronary tablet specific chromatogram and measuring six components | |
| CN106728651A (en) | The preparation method and its method of quality control of a kind of rhizoma cyperi SIWU KELI | |
| CN106370751A (en) | Traditional Chinese medicine composition fingerprint construction method and a detection method thereof | |
| CN105974025A (en) | Detection method of traditional Chinese preparation for treating stomach illness | |
| CN106706810B (en) | Novel biochemical particles quantitative finger print atlas detection method and its finger-print |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20221208 Address after: No.1 Guanqing Road, Guanlan hi tech park, Guanhu street, Longhua District, Shenzhen, Guangdong Province Patentee after: CHINA RESOURCES SANJIU MEDICAL & PHARMACEUTICAL Co.,Ltd. Patentee after: China Resources Sanjiu modern traditional Chinese Medicine Pharmaceutical Co.,Ltd. Address before: No.1 Guanqing Road, Guanlan high tech park, Longhua New District, Shenzhen, Guangdong 518110 Patentee before: CHINA RESOURCES SANJIU MEDICAL & PHARMACEUTICAL Co.,Ltd. |